Treatment of wool grease



Patented Jan. 5, 1954 TREATMENT OF WooL GREASE John P. Stanley,Amsterdam, N. Y., assignor to Mohawk Carpet Mills, Inc.',

Amsterdam, N. Y.,

a corporation of New York No Drawing. Application March 22, 1950,

Serial No. 151,322

7 Claims.

This invention relates to the treatment of lanolin or wool grease andthe production of a product having improved emulsifying properties.

More particularly, the invention relates to an improved process in whichlanolin or wool grease is subjected to a limited and partial oxidationby treatment with chemical oxidizing agents such as sodium chlorite andsulfuric acid, etc., to produce products having improved emulsifyingproperties.

The usual methods of emulsifying lanolin or wool grease involve the useof added soaps or other emulsifying agents, or dissolving in a solventand then effecting the emulsification with a soap or emulsifying agent.

I have found that lanolin or wool grease can be converted into a readilyemulsifiable product by treatment with oxidizing agents and effecting alimited and partial oxidation thereof, and by adding a small amount ofalkali to the oxidized product.

The oxidation of the lanolin or wool grease is effected by chemicaloxidizing agents such as a mixture-of sodium chlorite and sulfuric'acid.

The invention Will be further illustrated by the following examples:

Example I .l kilos of crude (neutral) lanolin or 'wool grease are placedin a closed vessel provided with heating means and a stirrer and thereis added 1.5 liters of 10% tion-with stirring followed by the additionof 0.2 liter of 50% sulfuric acid. The whole mixture is then wellstirred and allowed to stand about 16 hours at room temperature (21-24C.) and then heated at 100 C. for about 1 hours. mixture is then washedwith water by'adding about twice as much water as there is of themixture with stirring and heating to above the melting point and thencooling, after which the water is drawn off. This washing treatment isrepeated three times. The resulting washed product is then heated to themelting point. Approximately 25 kilos of water containing sufficientpotassium hydroxide to make the resulting mixture with the wool greaseproduct alkaline to litmus is heated to approximately the sametemperature as the melting wool grease product and then poured into theproduct with thorough stirring. This results in a smooth emulsion of theoil-in-water type.

The amount of sodium chlorite and of sulfuric acid can be variedsomewhat and products varying somewhat in their emulsifying propertiesobtained. Thus, from about 0.04 part of sodium chlorite for each 10parts of wool grease .up to 2 parts of sodium chlorite for each 10 partsof sodium chlorite solu- 4 The'- wool grease have been tried and thebest results were obtained with the larger quantities. Similarly,various quantities of sulfuric acid were tried from about 0.1 part ofsulfuric acid for 10 parts of wool grease to 0.25 part of sulfuric acidfor 10 parts of wool grease, depending upon the amount of sodiumchlorite used and usually having enough acid present so that thereaction took place in an acid medium. Other acids, e. g., hydrochloricacid, can be used instead of sulfuric acid.

The process can be carried out at different temperatures and fordifferent periods of time, varying from room temperature to around C.and from around 16 hours to hour for the chlorite treatment.

Example II.-10 kilos of wool grease are treated with 6.5 liters of 10%sodium chlorite solution which are stirred into the wool grease and then0.35 liter of l 50% sulfuric acid are added and stirred in andthereaction is allowed to proceed at room temperature (2l-24= C.) for 1hour with intermittent stirring. The vessel is heated up to 100 C. for15 minutes after which the product is washed three times with water. Theproduct is then melted at a temperature of 40*50 C. and 25 liters of 1%sodium carbonate solution previously heated to 40-50 C. are added andstirred in, with resulting formation of a good emulsion.

Various kinds and strengths of alkali were tried and it was found thatin general there should be sufiicient alkali present to make the wholeproduct alkaline. Thus, potassium hydroxide, sodium hydroxide, sodiumcarbonate, ammonium hydroxide; sodium borate, and triethanolamine wereall used as additions to the product resulting from the treatment of thewool grease or lanolin with sodium chlorite and acid. A 1% solution ofsodiumcarbonate is advantageously used.

In the processes of the above examples chlorine dioxide is formed as anoxidizing agent. When chlorine dioxide gas is used or is formed duringthe reaction a closed vessel is advantageously used.

The action of the limited and partial oxidation treatment of the lanolinor wool grease is to increase substantially the free acidity. Thus, whenwashed U. S. P. lanolin having an initial acidity of oleic acid of 0.98was treated in a manner similar to that indicated in Example II abovethe oxidized product had an acid value of about 1.8%. When treated againwith the same quantities of sodium chlorite and sulfuric acid theacidity increased to about 5.75 A similar treatment with an increasedamount of sodium chlorite equal to one-fifth the weight of the woolgrease and with twice the amount of sulfuric acid used in Example IIgave a product having an acid value of about 3.97%. All of theseproducts were readily emulsifiable, those with higher acidities havingsomewhat better emulsifying properties. Other changes, other than theincrease in acidity, also appear to be brought about by the limited andpartial oxidation. A slight decrease has been observed in thesaponification number of the treated product as compared with theproduct before treatment. The presence of the increased amount of freeacids produced by the oxidation treatment results in the formation ofsalts or soaps with the added alkali and gives a product having improvedemulsifying properties.

In the process illustrated by the above examples an emulsion is usuallyformed in the treatment as the chlorite and acid are in aqueous solutionand are mixed in with the lanolin, and the reaction product was washedwith water. The process can be somewhat improved by breaking anyemulsion that remains at the end of the process prior to washing toremove the inorganic acids and salts. One method of doing this is todissolve the product in a solvent such as ethyl ether, ethylenedichloride or chloroform, then washing the solution with water andsubsequently separating the solution and evaporating the solvent anddrying the product. A centrifugal method of breaking or separating theemulsion can also be used.

The oxidized lanolin or wool grease product resulting from the limitedand partial oxidation treatment contains an increased amount of freeacids resulting from the oxidation treatment and is an improvedemulsifiable product. It can readily be converted into an emulsion bythe addition of water containing sufficient alkali to make the resultingproduct slightly alkaline although in some cases an excess of alkali, e.g., sodium carbonate, may be present.

It is one advantage of the new lanolin or wool grease product, resultingfrom treatment with oxidizing agents, that the products are emulsifiablewithout the addition of soaps or emulsifying agents, and that emulsionscan be prepared therefrom simply by the addition of weak alkalinesolutions. As a result the emulsifying process is more flexible andadjustments can readily be made in the solids content of the emulsions.Another important advantage of the product is that it is more easilysaponified when it is desired to separate the acids and alcoholscontained in the oxidized products for the production, e. g'., ofcholesterol and wool fat acids including acids formed by the partialoxidation treatment.

Iclaim: I

1. The method of treating lanolin or wool grease to improve theemulsification properties thereof which comprises subjecting the same toa limited and partial oxidation treatment with an aqueous acid chloriteoxidizing agent and continuing such oxidation treatment until there isan increase of from about 9.82% to 4.77% in the free acidity and to givean oxidized product which, after washing with water, forms emulsions onthe addition of weak aqueous alkaline solutions.

2. The process according to claim 1 in which the treatment is with amixture of a solution of sodium chlorite and of sulfuric acid.

3. The method according to claim 1 in which the oxidized product isWashed with water.

4. The process according to claim 1 in which the product after washingis emulsified with a dilute alkaline solution sufficient in amount togive an emulsion with an alkaline reaction.

5. The process according to claim 1 in which the product after washingis emulsified and saponified with an alkaline solution to separate thealcohols from the acids.

6. The method of treating lanolin or wool grease to improve theemulsification properties thereof which comprises subjecting the same toa limited and partial oxidation treatment with an aqueous solution ofsodium chlorite and sulfuric acid, continuing such oxidation treatmentto effect an increase of from about 0.82% to 4.77% in the free acidity,washing the resulting product with Water, and preparing an emulsiontherefrom by the addition of a dilute alkaline solution sufficient inamount to give an emulsion with an alkaline reaction.

7. An oxidized lanolin or wool grease product containing from about 1.8%to 5.75% of acids resulting from a limited and partial oxidationtreatment thereof with an aqueous acid chlorite solution, said productforming oil-in-water emulsions on the addition thereto of a diluteaqueous alkaline solution.

JOHN P. STANLEY.

References Cited in the file of this patent UNITED STATES PATENTS NumberName Date 2,473,930 Woodward June 21, 1949 2,481,463 Woodward Sept. 6,1949 FOREIGN PATENTS Number Country Date 214,937 Germany of 1906 386,715Great Britain of 1933 OTHER REFERENCES Chem. Abst. 35-6348

1. THE METHOD OF TREATING LANOLIN OR WOOL GREASE TO IMPROVE THEEMULSIFICATION PROPERTIES THEREOF WHICH COMPRISES SUBJECTING THE SAME TOA LIMITED AND PARTIAL OXIDATION TREATMENT WITH AN AQUEOUS ACID CHLORITEOXIDIZING AGENT AND CONTINUING SUCH OXIDATION TREATMENT UNTIL THERE ISAN INCREASE OF FROM ABOUT 0.82% TO 4.77% IN THE FREE ACIDITY AND TO GIVEAN OXIDIZED PRODUCT WHICH, AFTER WASHING WITH WATER, FORMS EMULSIONS ONTHE ADDITION OF WEAK AQUEOUS ALKALINE SOLUTIONS.